Mangelings Debby, Tanret Indiana, Matthijs Nele, Maftouh Mohamed, Massart D Luc, Vander Heyden Yvan
Department of Pharmaceutical and Biomedical Analysis, Pharmaceutical Institute, Vrije Universiteit Brussel-VUB, Brussels, Belgium.
Discovery Analytical Department, Sanofi-Synthelabo Recherche, Toulouse, France.
Electrophoresis. 2005 Feb;26(4-5):818-832. doi: 10.1002/elps.200410190.
The effect of five factors on the capillary electrochromatographic enantioseparation of acidic compounds was studied using an experimental design. The studied factors were pH, acetonitrile content in the mobile phase, temperature, buffer concentration, and applied voltage. These experiments allowed defining a generic separation strategy applicable on acidic compounds with chemical and structural diversity. The starting screening conditions consist of a 45 mM ammonium formate electrolyte at pH 2.9 mixed with 65% acetonitrile, an applied voltage of 15 kV, and a temperature of 25 degrees C. The screening phase occasionally can be followed by an optimization procedure. Evaluation of the proposed strategy pointed out that it allows achieving baseline resolution within a relatively short time when a beginning of separation is obtained at the starting conditions. This strategy revealed enantioselectivity for 11 compounds out of 15, of which 10 could be baseline-separated after the proposed optimization steps.
采用实验设计研究了五个因素对酸性化合物毛细管电色谱对映体分离的影响。所研究的因素为pH值、流动相中乙腈含量、温度、缓冲液浓度和施加电压。这些实验确定了一种适用于具有化学和结构多样性的酸性化合物的通用分离策略。初始筛选条件包括pH 2.9的45 mM甲酸铵电解质与65%乙腈混合、15 kV的施加电压和25℃的温度。筛选阶段偶尔可接着进行优化程序。对所提出策略的评估指出，当在起始条件下实现分离起始时，该策略能够在相对较短的时间内实现基线分离。该策略对15种化合物中的11种显示出对映选择性，其中10种在经过所提出的优化步骤后可实现基线分离。
